CN103589010A - Microporous wave-absorbing material with low surface density and high tensile strength and preparation method - Google Patents
Microporous wave-absorbing material with low surface density and high tensile strength and preparation method Download PDFInfo
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Abstract
The invention discloses a microporous wave-absorbing material with low surface density and high tensile strength and a preparation method and belongs to the technical field of wave-absorbing material. According to the invention, problems of high density, low mechanical properties and poor temperature resistance of a present microwave material are solved. The preparation method comprises steps of: uniformly stirring rubber, zinc oxide, eleaostearic acid, an anti-aging agent, a flow promoter, sulphur, a promoter, a foaming agent, a plasticiser and an absorbent, banburying, open-milling, vulcanizing at 150-160 DEG C and simultaneously foaming for 25-35min so as to obtain the microporous wave-absorbing material. The total thickness of the prepared microporous wave-absorbing material is between 1.4mm and 2.0mm, and its surface density is less than 1.7kg/m<2>. The material has good wave-absorbing performance at specific wavelengths. Meanwhile, the material has good temperature resistance and mechanical property. The temperature that the material resists can reach 150 DEG C. Average value of tensile strength is greater than 8.5MPa, and the minimum elongation at break is 360%.
Description
Technical field
The present invention relates to micropore absorbing material of a kind of low area density high tensile and preparation method thereof, belong to absorbing material technical field.
Background technology
In prior art, patch-type absorbing material is generally to adopt tackiness agent to mix roll-in with absorption agent (being generally magneticsubstance) to form.By selecting different base materials, optimization of C/C composites design, makes the performance of absorbing material meet different demands.This class patch-type material is inhaled ripple and is had the advantages such as good uniformity, process controllability is strong, material property (particularly electrical property) is stable, construction technology is simple.
But, the too high shortcoming of existing patch-type absorbing material ubiquity area density, thickness has surpassed 3.0kg/m mostly less than its area density of suction wave plate of 1mm
2, intensity is generally in 4MPa left and right, and heat resistance, generally lower than 100 ℃, cannot meet the requirements such as mechanical property of the equipments such as aircraft.
Summary of the invention
The object of the invention is in order to solve the problem that existing absorbing material area density is large, mechanical property is low and heat resistance is bad, and absorbing material of a kind of low area density high tensile and preparation method thereof is provided.
The micropore absorbing material of low area density high tensile of the present invention, comprises rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent, fluidizer and absorption agent; The mass ratio of described rubber, whipping agent and fluidizer is 100:(5-18): (15-25); Described whipping agent is Cellmic C 121 (AC), modification Cellmic C 121 (ACPW) or N, N'-dimethyl five methyne tetramines; Described absorption agent is micron order graphitized carbon black, and the quality of absorption agent is the 30-40% of the total mass of rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent and fluidizer.
Preferably, the quality of described absorption agent is the 5-18% of the total mass of rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent and fluidizer.
Preferably, the mass ratio of described rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur and promotor is 100:5:2:2:1.5:2:1.
Preferably, described rubber is paracril or hydrogenated nitrile-butadiene rubber.
Preferably, described anti-aging agent is N, N-nickel dibutyl dithiocarbamate (NBC), 2,2,4-trimethylammonium-1, one or more in 2-dihyaroquinoline polymer (RD), N-sec.-propyl-N'-diphenyl-para-phenylene diamine (4010NA).
Preferably, described flow promotor is particulate state lipid acid, particulate state derivative of fatty acid or particulate state stearic acid isoamyl tetrol.
Preferably, described promotor is N-cyclohexyl-2-benzothiazole sulfonamide (CZ) or 2-benzothiazolyl mercaptan (MBT).
Preferably, described fluidizer is one or more in dibutyl phthalate, dioctyl phthalate (DOP), diethyl phthalate.
The preparation method of the micropore absorbing material of above-mentioned low area density high tensile, comprises the following steps:
(1) after rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent, fluidizer and absorption agent are stirred, banburying mixes, and obtains mixture;
(2) mixture step (1) being obtained is opened refining to the raw material that obtains stable homogeneous;
(3) raw material of stable homogeneous step (2) being obtained, at 150-160 ℃ of sulfuration the 25-35min that foams simultaneously, obtains the micropore absorbing material of low area density high tensile.
Preferably, in step (1), described banburying be in Banbury mixer 85 ℃ with interior banburying 10-15min, in step (2), described in open refining be in mill, open refining more than 20 times.
Beneficial effect of the present invention:
(1) the present invention adopts micron order graphitized carbon black as absorption agent, has lower area density when making material have excellent absorbing property, and provides certain strengthening action to material, further increases the mechanical property of material; And adopt and the whipping agent of sulfuration in same temperature interval, when being vulcanized in preparation process, material foams, and guaranteed that the distribution of cells of material is even, and there is unicellular structure, realized low density and the high strength of material;
(2) the micropore absorbing material total thickness that prepared by the present invention is between 1.4-2.0mm, and area density is less than 1.7kg/m
2, material has good absorbing property at specific band, has good temperature tolerance and mechanical property simultaneously, and heatproof can reach 150 ℃, and tensile strength mean value is greater than 8.5MPa, and elongation at break minimum value is 360%;
(3) preparation method of the present invention foaming in material sulfuration, has not only guaranteed the structure of microwave material, and simple, easily row, cost are low, are beneficial to scale operation.
Accompanying drawing explanation
Fig. 1 is the flat reflective rate test curve figure of the micropore absorbing material material prepared of embodiment of the present invention 1-3;
In Fig. 2, (a) be the opticmicroscope image of the micropore absorbing material cross section of the embodiment of the present invention 1 preparation; (b) be the opticmicroscope image of the micropore absorbing material cross section of the embodiment of the present invention 2 preparations.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiments of the invention are described, but should be appreciated that these are described is the restriction for further illustrating the features and advantages of the present invention rather than patent of the present invention being required.
The micropore absorbing material of low area density high tensile comprise the rubber of 100 weight parts, the stearic acid of the zinc oxide of 5 weight parts, 2 weight parts, the flow promotor of the anti-aging agent of 2 weight parts, 1.5 weight parts, the promotor of the sulphur of 2 weight parts, 1 weight part, fluidizer and the absorption agent of the whipping agent of 5-18 weight part, 15-25 weight part; Wherein, rubber is paracril 220 or hydrogenated nitrile-butadiene rubber; Anti-aging agent is N, N-nickel dibutyl dithiocarbamate, 2,2,4-trimethylammonium-1, in 2-dihyaroquinoline polymer, N-sec.-propyl-N'-diphenyl-para-phenylene diamine one or more; Flow promotor is particulate state lipid acid, particulate state derivative of fatty acid or particulate state stearic acid isoamyl tetrol, preferred particulates shape derivative of fatty acid ZC-56 or particulate state stearic acid isoamyl tetrol D-821; Promotor is N-cyclohexyl-2-benzothiazole sulfonamide or 2-benzothiazolyl mercaptan; Fluidizer is one or more in dibutyl phthalate, dioctyl phthalate (DOP), diethyl phthalate; Whipping agent is Cellmic C 121, modification Cellmic C 121 or N, N'-dimethyl five methyne tetramines; Absorption agent is micron order graphitized carbon black, its quality is the 30-40% of the total mass of rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent and fluidizer, preferred 5-18% (known according to field, the noresidue after forming the finished product of acquiescence whipping agent is calculated).
The preparation method of the micropore absorbing material of low area density high tensile, comprises the steps:
(1) after rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent, fluidizer and absorption agent physical agitation is even, add banburying in Banbury mixer to mix, obtain mixture;
Described rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, the mass ratio of whipping agent and fluidizer is 100:5:2:2:1.5:2:1:(5-18): (15-25), described whipping agent is Cellmic C 121, modification Cellmic C 121 or N, N'-dimethyl five methyne tetramines, described absorption agent is micron order graphitized carbon black, its quality is rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, the 30-40% of the total mass of whipping agent and fluidizer, preferably 5-18% is (known according to field, the noresidue after forming the finished product of acquiescence whipping agent is calculated),
(2) mixture step (1) being obtained adds in mill, to wrap the technique of roller, opens refining, obtains the raw material of stable homogeneous;
(3) raw material of stable homogeneous step (2) being obtained adds in mould, and mould is placed in to vulcanizing press, at 150-160 ℃ of sulfuration the 25-35min that foams simultaneously, cuts out and removes unnecessary rim charge, obtains the micropore absorbing material of low area density high tensile.
In the present invention, rubber is paracril 220 or hydrogenated nitrile-butadiene rubber, anti-aging agent is N, N-nickel dibutyl dithiocarbamate, 2, 2, 4-trimethylammonium-1, 2-dihyaroquinoline polymer, in N-sec.-propyl-N'-diphenyl-para-phenylene diamine one or more, flow promotor is particulate state lipid acid, particulate state derivative of fatty acid ZC-56 or particulate state stearic acid isoamyl tetrol D-821, preferred particulates shape derivative of fatty acid ZC-56 or particulate state stearic acid isoamyl tetrol D-821, promotor is N-cyclohexyl-2-benzothiazole sulfonamide or 2-benzothiazolyl mercaptan, fluidizer is dibutyl phthalate, dioctyl phthalate (DOP), one or more in diethyl phthalate.
In step of the present invention (1), the order of addition of rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent, fluidizer and absorption agent has certain requirement, according to field, personnel are known, for preventing that excess Temperature from producing sulfuration in advance, sulphur and promotor will in the end add.
In step of the present invention (1), in order to prevent auxiliary agent, at high temperature effective constituent is destroyed, and banburying process temperature is preferably controlled in 85 ℃.
In step of the present invention (2), rubber is opened sweetening process owing to joining glue amount, according to existing refining glue three guarantees two roller techniques, can not make it fully open refining evenly, therefore, preferably uses 20 the above methods of refining of opening.
The kind of Banbury mixer used in the present invention and mill is selected according to the amount of preparing absorbing material.
Plate vulcanization machine die size used herein 200 * 200mm
2or 300 * 300
2mm, more preferably 300 * 300
2mm, die cavity height dimension capable of regulating changes according to demand between 1.0-2.0mm.
Below in conjunction with embodiment and accompanying drawing, the present invention is done to further detailed description.
Embodiment 1
By 100g paracril 220,5g zinc oxide, 2g stearic acid, 2gN, N-nickel dibutyl dithiocarbamate, 1.5g particulate state lipid acid, 2g sulphur, 1gN-cyclohexyl-2-benzothiazole sulfonamide, 5g Cellmic C 121,15g dibutyl phthalate and 40.5g micron order graphitized carbon black add in Banbury mixer 85 ℃ with interior banburying, to mix, and obtain mixture; The mixture that banburying is obtained moves to mill and opens refining and obtain the raw material of stable homogeneous, then 62.0g raw material is cut into suitable dimension puts into 200 * 200
2in the mould of mm, die cavity height dimension 1.2mm, at 150 ℃ in vulcanizing press sulfur foam 25min, obtain micropore absorbing material, the mechanical property of material is as shown in table 1.
Embodiment 2
By 100g paracril 220,5g zinc oxide, 2g stearic acid, 2g2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer, 1.5g particulate state derivative of fatty acid ZC-56,2g sulphur, 1g2-benzothiazolyl mercaptan, 10g modification Cellmic C 121,20g dioctyl phthalate (DOP) and 50.225g micron order graphitized carbon black add banburying in Banbury mixer to mix, and obtain mixture; The mixture that banburying is obtained moves to mill and opens refining and obtain the raw material of stable homogeneous, then 65.0g raw material is cut into suitable dimension puts into 200 * 200
2in the mould of mm, die cavity height dimension 1.5mm, at 155 ℃ in vulcanizing press sulfur foam 30min, obtain micropore absorbing material, the mechanical property of material is as shown in table 1.
Embodiment 3
By 100g hydrogenated nitrile-butadiene rubber, 5g zinc oxide, 2g stearic acid, 1gN-sec.-propyl-N'-diphenyl-para-phenylene diamine, 1gN, N-nickel dibutyl dithiocarbamate, 1.5g particulate state stearic acid isoamyl tetrol D-821,2g sulphur, 1g2-benzothiazolyl mercaptan, 15gN, N'-dimethyl five methyne tetramines, 20g dioctyl phthalate (DOP), 3g diethyl phthalate and 50.3275g micron order graphitized carbon black add banburying in Banbury mixer to mix, and obtain mixture; The mixture that banburying is obtained moves to mill and opens refining and obtain the raw material of stable homogeneous, then 71.0 raw materials are cut into suitable dimension put into 200 * 200
2in the mould of mm, die cavity height dimension 1.7mm, at 155 ℃ in vulcanizing press sulfur foam 35min, obtain micropore absorbing material.
The micropore absorbing material of embodiment 1-2 is made into dumbbell specimen, width 6mm, operating range 25mm.Mechanics Performance Testing equipment is that the SUNS electronic universal tester of Science and Technology Co., Ltd. is in length and breadth thought carefully in Shenzhen, and GB/T528-1998 vulcanized rubber drawing process is used in test.Test result is in Table 1.
The mechanical property of the micropore absorbing material of table 1 embodiment 1 and embodiment 2
The micropore absorbing material that embodiment 1-3 is obtained cuts into 180 * 180mm
2standard sample of photo, the RCS testing apparatus of material is the N-5244A of Agilent vector network analyzer PNA-X series, testing method is arc method, for 8-12GHz frequency range, tests.Test result as shown in Figure 1.Material is carried out to longitudinal section and cut, obtain horizontal section, utilize electron microscope to carry out section structure shooting, obtain its foaming size and foaming distribution situation.Test result is as Fig. 2.
Curve in Fig. 1 (a) is the flat reflective rate of the micropore absorbing material of embodiment 1, from curve (a), can find out, material absorbs all lower than-6dB in 8-12GHz band limits, peak value can reach-below 30dB; Curve in Fig. 1 (b) is the flat reflective rate of the micropore absorbing material of embodiment 2, from curve (b), can find out, material absorbs all lower than-7dB in 8-12GHz band limits, peak value can reach-below 25dB; Curve in Fig. 1 (c) is the flat reflective rate of the micropore absorbing material of embodiment 3, from curve (c), can find out, material absorbs all lower than-7.5dB in 8-12GHz band limits, peak value can reach-and below 25dB.
Fig. 2 (a) is the cross section opticmicroscope image of the micropore absorbing material of embodiment 1, as can be seen from the figure material foaming distribution uniform, and the diameter of closed pore is 100 microns of left and right; Fig. 2 (b) is the cross section opticmicroscope image of the micropore absorbing material of embodiment 2, and as can be seen from the figure, 100 microns, the foaming closed pore aperture of microwave material is in the majority, and maximum value reaches more than 200 microns.
Obviously, the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that the those of ordinary skill for described technical field, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (10)
1. the micropore absorbing material of low area density high tensile, is characterized in that, comprises rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent, fluidizer and absorption agent;
The mass ratio of described rubber, whipping agent and fluidizer is 100:(5-18): (15-25);
Described whipping agent is Cellmic C 121, modification Cellmic C 121 or N, N'-dimethyl five methyne tetramines;
Described absorption agent is micron order graphitized carbon black, and the quality of absorption agent is the 30-40% of the total mass of rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent and fluidizer.
2. the micropore absorbing material of low area density high tensile according to claim 1, it is characterized in that, the quality of described absorption agent is the 5-18% of the total mass of rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent and fluidizer.
3. the micropore absorbing material of low area density high tensile according to claim 1, is characterized in that, the mass ratio of described rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur and promotor is 100:5:2:2:1.5:2:1.
4. the micropore absorbing material of low area density high tensile according to claim 1, is characterized in that, described rubber is paracril or hydrogenated nitrile-butadiene rubber.
5. the micropore absorbing material of low area density high tensile according to claim 1, is characterized in that, described anti-aging agent is N, N-nickel dibutyl dithiocarbamate, 2,2,4-trimethylammonium-1, in 2-dihyaroquinoline polymer, N-sec.-propyl-N'-diphenyl-para-phenylene diamine one or more.
6. the micropore absorbing material of low area density high tensile according to claim 1, is characterized in that, described flow promotor is particulate state lipid acid, particulate state derivative of fatty acid or particulate state stearic acid isoamyl tetrol.
7. the micropore absorbing material of low area density high tensile according to claim 1, is characterized in that, described promotor is N-cyclohexyl-2-benzothiazole sulfonamide or 2-benzothiazolyl mercaptan.
8. the micropore absorbing material of low area density high tensile according to claim 1, is characterized in that, described fluidizer is one or more in dibutyl phthalate, dioctyl phthalate (DOP), diethyl phthalate.
9. the preparation method of the micropore absorbing material of the low area density high tensile of claim 1-8 described in any one, is characterized in that, comprises the following steps:
(1) after rubber, zinc oxide, stearic acid, anti-aging agent, flow promotor, sulphur, promotor, whipping agent, fluidizer and absorption agent are stirred, banburying mixes, and obtains mixture;
(2) mixture step (1) being obtained is opened refining to the raw material that obtains stable homogeneous;
(3) raw material of stable homogeneous step (2) being obtained, at 150-160 ℃ of sulfuration the 25-35min that foams simultaneously, obtains the micropore absorbing material of low area density high tensile.
10. the preparation method of the micropore absorbing material of low area density high tensile according to claim 9, it is characterized in that, in step (1), described banburying be in Banbury mixer 85 ℃ with interior banburying 10-15min, in step (2), described in open refining be in mill, open refining more than 20 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105400018A (en) * | 2015-12-21 | 2016-03-16 | 中国科学院长春应用化学研究所 | Microporous wave-absorbing material with array-structure surface, and preparation method thereof |
| CN115490934A (en) * | 2022-09-21 | 2022-12-20 | 中国热带农业科学院农产品加工研究所 | Double-loss rubber wave-absorbing material and rubber wave-absorbing body with ultra-wide-band absorption characteristic |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106959438A (en) * | 2017-03-29 | 2017-07-18 | 中国电子科技集团公司第三十八研究所 | A kind of TR assembly encapsulation structures |
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| CN105400018A (en) * | 2015-12-21 | 2016-03-16 | 中国科学院长春应用化学研究所 | Microporous wave-absorbing material with array-structure surface, and preparation method thereof |
| CN115490934A (en) * | 2022-09-21 | 2022-12-20 | 中国热带农业科学院农产品加工研究所 | Double-loss rubber wave-absorbing material and rubber wave-absorbing body with ultra-wide-band absorption characteristic |
| CN115490934B (en) * | 2022-09-21 | 2024-01-23 | 中国热带农业科学院农产品加工研究所 | Double-loss rubber wave-absorbing material and rubber wave-absorbing body with ultra-wideband absorption characteristic |
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